Ethanolamine → 2,2-Dichloro-1-(8-methyl-1-oxa-4-azaspiro[4.5]decan-4-yl)ethan-1-one

HRID 127484

反応式

HRID 127484 の反応式
[CH3:1][CH:2]1[CH2:7][CH2:6][C:5](=[O:8])[CH2:4][CH2:3]1.[CH2:9]([CH2:11][NH2:12])O.N1C=CC=CC=1.[Cl:19][CH:20]([Cl:24])[C:21](Cl)=[O:22]>>[Cl:19][CH:20]([Cl:24])[C:21]([N:12]1[C:5]2([CH2:6][CH2:7][CH:2]([CH3:1])[CH2:3][CH2:4]2)[O:8][CH2:9][CH2:11]1)=[O:22]

参加物

5

反応物 4

HCID 700EthanolamineHCID 1049PyridineHCID 6593Dichloroacetyl chlorideHCID 115254-Methylcyclohexanone

生成物 1

HCID 132772042,2-Dichloro-1-(8-methyl-1-oxa-4-azaspiro[4.5]decan-4-yl)ethan-1-one

実験手順

From a boiling mixture of 11.2 g. (0.1 moles) of 4-methyl-cyclohexanone and 6.1 g. (0.1 moles) of ethanolamine in 100 ml. of benzene the formed water is continuously distilled off. Boiling is continued until 1.8 ml. of water are separated. The reaction mixture is then cooled and 8 g. (0.1 moles) of pyridine are added followed by dropwise addition of 14.7 g. (0.1 moles) of dichloroacetyl chloride with external salt/ice cooling. Further following the procedure described in Example 2, 20.7 g. (0.078 moles) of a rose, oily product are obtained. Recrystallization from absolute ethanol affords a white, crystalline product melting at 119° to 120° C. The structure of the compound obtained can be verified by IR spectrum analysis.

後処理

  1. additionFrom a boiling mixture of 11.2 g
  2. distillationof benzene the formed water is continuously distilled off
  3. customof water are separated
  4. temperatureThe reaction mixture is then cooled
  5. additionfollowed by dropwise addition of 14.7 g
  6. customoily product are obtained
  7. customRecrystallization from absolute ethanol

出典と根拠

ORDレコード
ord-7e8eee49de1241f0a4981066e19cc3e7
出典データセット
uspto-grants-1981_03
特許番号
US04256481

関連ノート

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